4-BROMO-2-PIPERIDINOBENZENECARBALDEHYDE

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4-bromo-2-fluorobenzaldehyde (3.0 g), piperidine (2.93 ml) and potassium carbonate (5.11 g) in N,N-dimethylformamide (30 ml) was stirred at 100° C. for 12 hours. The mixture was cooled to room temperature. The mixture was partitioned between ethyl acetate and water. The organic layer was separated, washed with water, saturated aqueous ammonium chloride solution and brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=9/1) to give 4-bromo-2-(1-piperidinyl)benzaldehyde (3.5 g). The mixture was cooled to room temperature The mixture was partitioned between ethyl acetate and water The organic layer was separated washed with water, saturated aqueous ammonium chloride solution and brine dried over magnesium sulfate evaporated under reduced pressure The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=9/1)

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4-bromo-2-fluorobenzaldehyde (3.0 g), piperidine (2.93 ml) and potassium carbonate (5.11 g) in N,N-dimethylformamide (30 ml) was stirred at 100° C. for 12 hours. The mixture was cooled to room temperature. The mixture was partitioned between ethyl acetate and water. The organic layer was separated, washed with water, saturated aqueous ammonium chloride solution and brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=9/1) to give 4-bromo-2-(1-piperidinyl)benzaldehyde (3.5 g). The mixture was cooled to room temperature The mixture was partitioned between ethyl acetate and water The organic layer was separated washed with water, saturated aqueous ammonium chloride solution and brine dried over magnesium sulfate evaporated under reduced pressure The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=9/1)